CN106872560A - The device of each component and application in a kind of quantitative analysis alkene admixture of isomeric compound - Google Patents
The device of each component and application in a kind of quantitative analysis alkene admixture of isomeric compound Download PDFInfo
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- CN106872560A CN106872560A CN201510917247.4A CN201510917247A CN106872560A CN 106872560 A CN106872560 A CN 106872560A CN 201510917247 A CN201510917247 A CN 201510917247A CN 106872560 A CN106872560 A CN 106872560A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
Abstract
The invention provides a kind of apparatus and method of each component in quantitative analysis alkene admixture of isomeric compound, quantitative analysis device used includes the online preparation system of gaseous mixture, olefinic double bonds oxidative system and reaction stream outlet detecting system.The quantitative analysis method is the gaseous mixture that several olefins isomer is obtained using the online preparation system of above-mentioned gaseous mixture, then there is double bond oxidation reaction with ozone in olefinic double bonds oxidative system, a part for reaction stream outlet obtains the oxidation product feature spectrogram of alkene admixture of isomeric compound into the analysis of reaction stream outlet detecting system by the road, is finally based on the intensity at characteristic ion peak and species realizes the quantitative analysis of each component in mixture.In the process, real-time online prepares the gaseous mixture of alkene isomer, can shorten sample gas preparation time, and the efficiency of quantitative analysis can be greatly improved using quantitative analysis procedure.The quantified system analysis and method are simple to operate, quantitative accurate.
Description
Technical field
The present invention relates to a kind of apparatus and method of each component in quantitative analysis alkene admixture of isomeric compound, it is exactly specifically
The feature spectrogram of alkene isomer and its mixture is obtained using the quantified system analysis, the spy of each olefin component is then based on
Ionic strength is levied, the accurate quantitative analysis of each component in mixture are realized using quantitative analysis procedure.
Background technology
Long-chain olefin (long-chain olefins) is a kind of important Organic Ingredients and intermediate product, is widely used in surface
Activating agent, plasticizer, auxiliary agent and fine chemicals etc..The production of China's linear alkene be mainly with wax destructive distillation, ethylene oligomerization and
Based on linear paraffin catalytic dehydrogenation device.The product of linear alkanes dehydrogenation is sufficiently complex, there is alkene in alpha-olefin and straight chain in product
Hydrocarbon, linear internal position of double bond is different, there is many isomers.How alkene species i.e. position of double bond, and accurate quantitative analysis are determined
Concentration of olefin, for optimization catalyst composition and reaction condition, improves conversion ratio, reduces accessory substance, particularly significant.And it is current
Research majority on alkene or unrighted acid in document report is to explore the method for determining intramolecular position of double bond, such as high score
Distinguish capillary chromatography GC, GC-MS, H NMR spectroscopy method and a series of chemical derivatization methods.It is few to divide on quantitative
The report of isomerism alkene in analysis mixture.
The purpose of this paper is the new method for providing each component in a kind of quantitative analysis alkene admixture of isomeric compound.The method is smelly
Oxygen solution derivative reaction, by the olefin oxidation of different position of double bond, is single photon ionization mass spectrum using reaction stream outlet detecting system
Instrument carries out ionization detection, obtains the feature spectrogram of each olefin oxidation product.The intensity at each characteristic ion peak is finally based on, is utilized
Quantitative analysis procedure carries out accurate quantitative analysis to each component in gaseous mixture.The method achieve each group in alkene admixture of isomeric compound
The accurate quantitative analysis for dividing.In addition, the device gas circuit is simple, and it is with low cost, it is easy to operation.
The content of the invention
Present invention aim at the device for providing each component in a kind of quantitative analysis alkene admixture of isomeric compound, it is characterised in that：
Including the online preparation system of gaseous mixture, olefinic double bonds oxidative system and reaction stream outlet detecting system；
The online preparation system of gaseous mixture includes feeder, olefin samples gas generating means and olefin samples gas mixing arrangement,
Olefinic double bonds oxidative system includes ozone generating-device and ozonolysis reactions device；
Wherein, feeder includes oxygen source, the gas vent of oxygen source respectively with the gas access of ozone generating-device and
Two carrier gas inlets of the olefin samples gas generation device of more parallel are connected, and in oxygen source and ozone generating-device and two
The first mass flow controller is equipped with every pipeline between the olefin samples gas generation device of more parallel；
The ozone outlet of ozone generating-device is connected with the gas access of ozonolysis reactions device, two alkene of more parallel
The gas vent of sample gas generating means divides through olefin samples gas mixing arrangement and the second mass flow controller after being connected with ozone
The gas access for solving reaction unit is connected, and gas vent and the gas of reaction stream outlet detecting system of ozonolysis reactions device enter
Sample mouthful is connected.
The ozonolysis reactions device is the ozone outlet and alkene of copper pipe or stainless steel tube, its one end and ozone generating-device
The gas vent of sample gas generating means is connected, and the other end is connected with the gas sampling mouthful of reaction stream outlet detecting system；
The olefin samples gas generating means at least two, is a hollow airtight cavity with heating element heater, hollow closed
What cavity was provided with fluid sample bottle is removed and placed into mouth, and fluid sample bottle is removed and placed into mouth and can be opened and closed by one
Lid it is closed, fluid sample bottle be placed in hollow airtight cavity.
The ozonolysis reactions device length is adjustable, and profile is screw type or U-shape structure, is easy to ozone and long-chain olefin sample
Product gas is sufficiently mixed reaction；
Heating element heater is electrical heating wire, heat tape or electrical heating block；
Olefin samples gas generating means is the stainless steel cylinder with stainless steel bottle cap, and stainless steel bottle cap and stainless steel body pass through screw thread
Fasten, and sealing is enclosed using O, inside holds fluid sample bottle.
Oxygen source is the dry air after steel cylinder or purification equipped with oxygen；
The unstripped gas that ozone generating-device is used to produce ozone gas is pure oxygen high or dry air, and the concentration that ozone is obtained can pass through
Adjust the uninterrupted regulation of the size of current and unstripped gas of corona discharge type ozone generating-device.
The reaction stream outlet detecting system is the analytical equipment of direct gas sampling, predominantly the on-line mass spectroscopy instrument of gas sampling,
It is connected with ozonolysis reactions device by gas sampling pipe；Ozonolysis reactions are flowed out with a part of sampling analysis of gas, remaining
Discharged as tail gas.
The cavity size of the olefin samples gas generating means can be with the size adjustment of olefin samples bottle, and cavity heating-up temperature can be with root
Set according to the concentration of required alkene.
The olefin samples gas mixing arrangement is copper pipe or stainless steel tube, and adjustable length is spiral-shaped structure, is easy to isomerism
Olefin samples gas is sufficiently mixed；
Isomerism olefin samples gas be sufficiently mixed after through the second mass flow controller shunting, be partly into ozone decomposed anti-
Device is answered, remaining is discharged as tail gas.
Operated using any described device in claim 1-7, comprised the following steps：
A. the olefin samples bottle of more than two is respectively put into two olefin samples gas generating means of more parallel, sets alkene
The heating-up temperature and gas flow of hydrocarbon samples gas generating means, open two olefin samples gas generating means of more parallel respectively
First mass flow controller, respectively obtains certain density each olefin component sample gas；Divide in the olefin samples bottle of more than two
It is not contained with the one kind in alkene isomer to be detected, and is contained with respectively in the olefin samples bottle of more than two to be detected
Alkene isomer it is different；
B. setting is passed through the gas flow and size of current of ozone generating-device, prepares ozone；
C. each olefin component sample gas for step A being obtained respectively with ozone in ozonolysis reactions device hybrid reaction, together
Shi Liyong reaction stream outlet detecting systems obtain the feature spectrogram of each olefin component；
D. the olefin samples bottle that alkene admixture of isomeric compound to be detected will be contained with is respectively put into an olefin samples gas generation
In device, the first mass flow controller of olefin samples gas generating means is opened；
E. the size of the second mass flow controller is set, by above-mentioned steps D part gaseous mixtures and ozone in ozonolysis reactions
Hybrid reaction in device, while obtaining the feature spectrogram of olefine mixing gas using reaction stream outlet detecting system；
The sample gas concentration of each olefin component for F. being obtained using weight method determination step A, and it is calculated what step D was obtained
Olefine mixing gas concentration；
G. characteristic ion species and intensity based on each olefin component, quantitative calculating is carried out to each component in mixture.
The gas conduit is quartz capillary or stainless steel capillary；
The ozonolysis reactions device is the pipeline of stainless steel, and non-cohesive material, it is to avoid corruption of the ozone to reaction pipeline
Erosion.
Reaction stream outlet detecting system is online gas sampling mass spectrograph, and reaction stream outlet is entered using Single-photon ionization (SPI)
Row ionization, the method can simplify the spectrogram of ozonolysis product, be easy to spectrum elucidation.
The general principle of quantitative analysis procedure is：
Carried out with VUV light SPI ionization and ion-molecule reaction it is simultaneous during, certain characteristic ion M of alkene+
Intensity IM+(ions s-1) with the concentration C of alkeneN(molecules cm-2) can be represented with formula 1.
IM +=σequCN (1)
Wherein, σequEffective ionization coefficient is defined as, the ozone decomposed for describing long-chain olefin under specific condition of experiment converts effect
Rate and characteristic ion M+Ionizing efficiency, can be calculated by the alkene of concentration known and its corresponding ionic strength.So
And, often there is peak overlap phenomenon in the characteristic ion of isomer alkene, i.e., one or more characteristic ion peaks are both present in
In the long-chain olefin spectrogram of isomer, at this moment need to be quantified so that Accurate Determining is each same using multiple characteristic ions simultaneously
Divide the content of isomeric olefine.Therefore, the pass in admixture of isomeric compound between the concentration of each alkene and the intensity of its characteristic ion
System should be shown in formula 2.
Wherein, I (mn) it is characteristic ion m in actually measured admixture of isomeric compound spectrogramnIntensity, σj equ(mn) it is mixed
The characteristic ion m of olefin component j in compoundnEffective ionization coefficient, CjIt is the concentration of olefin component j in mixture.
The features of the present invention：
Because the intensity present invention employs various features ion carries out quantitative analysis to mixture each component, while by some features
The same source ion of ion is taken into account, therefore the degree of accuracy is high.The system architecture is simple simultaneously, and easy to operate, quantitative precision is high.
Brief description of the drawings
Fig. 1 is the system schematic of each component in quantitative analysis alkene admixture of isomeric compound；1- ozone generating-devices；2- alkene
Hydrocarbon samples gas generating means；3- ozonolysis reactions devices；4- feeders；5- reaction stream outlet detecting systems；6- pure oxygens high
Steel cylinder；7- the first precision mass flow controllers；16- the second precision mass flow controllers；8- vacuum UV lamps；9- gases are led
Pipe；10- ionized regions；11- vacuum plants；12- field-free flights area；13-MCP detectors；14- data collecting systems；15- tails
Gas；17- olefin samples gas mixing arrangements.
Fig. 2 is 3 kinds of ozonolysis product feature spectrograms of octene isomer；
Fig. 3 is 2 kinds of ozonolysis product feature spectrograms of octene admixture of isomeric compound；
Fig. 4 is the relative amount of each component in 2 kinds of octene mixtures that weight method and quantitative analysis procedure are obtained.
Specific embodiment
First, Fig. 1 is a kind of device of each component in quantitative analysis alkene admixture of isomeric compound, it is characterised in that：Including
The online preparation system of gaseous mixture, olefinic double bonds oxidative system and reaction stream outlet detecting system 5；
The online preparation system of gaseous mixture includes feeder 4, olefin samples gas generating means 2 and olefin samples gas mixing dress
17 are put, olefinic double bonds oxidative system includes ozone generating-device 1 and ozonolysis reactions device 3；
Wherein, feeder 4 includes oxygen source 6, the gas vent of oxygen source 6 respectively with the gas of ozone generating-device 1
Body entrance and two carrier gas inlets of the olefin samples gas generation device 2 of more parallel are connected, and are sent out in oxygen source 6 and ozone
The first mass flow control is equipped with every pipeline between generating apparatus 1 and two olefin samples gas generation devices 2 of more parallel
Device processed 7；
The ozone outlet of ozone generating-device 1 is connected with the gas access of ozonolysis reactions device 3, two more parallels
The gas vent of olefin samples gas generating means 2 is controlled after being connected through olefin samples gas mixing arrangement 17 and the second mass flow
Device 16 is connected with the gas access of ozonolysis reactions device 3, and gas vent and the reaction of ozonolysis reactions device 3 are flowed out
The gas sampling mouthful of gas detecting system 5 is connected.
The ozonolysis reactions device 3 is copper pipe or stainless steel tube, the ozone outlet of its one end and ozone generating-device 1 and
The gas vent of olefin samples gas generating means 2 is connected, and the other end is connected with the gas sampling mouthful of reaction stream outlet detecting system 5；
The olefin samples gas generating means 2 at least two, is a hollow airtight cavity with heating element heater, hollow close
What closed chamber body was provided with fluid sample bottle is removed and placed into mouth, and fluid sample bottle is removed and placed into mouth and can be opened and be closed by one
The lid for closing is closed, and fluid sample bottle is placed in hollow airtight cavity.
The adjustable length of ozonolysis reactions device 3, profile is screw type or U-shape structure, is easy to ozone and long-chain olefin sample
Product gas is sufficiently mixed reaction；
Heating element heater is electrical heating wire, heat tape or electrical heating block；
Olefin samples gas generating means 2 is the stainless steel cylinder with stainless steel bottle cap, and stainless steel bottle cap and stainless steel body pass through spiral shell
Line is fastened, and encloses sealing using O, and inside holds fluid sample bottle.
Oxygen source 6 is the dry air after steel cylinder or purification equipped with oxygen；
The unstripped gas that ozone generating-device 1 is used to produce ozone gas is pure oxygen high or dry air, and the concentration that ozone is obtained can lead to
Overregulate the uninterrupted regulation of the size of current and unstripped gas of corona discharge type ozone generating-device 1.
The reaction stream outlet detecting system 5 is the analytical equipment of direct gas sampling, the predominantly on-line mass spectroscopy instrument of gas sampling,
It is connected with ozonolysis reactions device 3 by gas sampling pipe 9；Ozonolysis reactions are flowed out with a part of sampling analysis of gas,
Remaining is discharged as tail gas 15.
The cavity size of the olefin samples gas generating means 2 can be with the size adjustment of olefin samples bottle, cavity heating-up temperature
Concentration setting according to required alkene.
The olefin samples gas mixing arrangement 17 is copper pipe or stainless steel tube, and adjustable length is spiral-shaped structure, is easy to same point
Isomeric olefine sample gas are sufficiently mixed；
Isomerism olefin samples gas be sufficiently mixed after through the second mass flow controller 16 shunting, be partly into ozone point
Solution reaction unit 3, remaining is discharged as tail gas 15.
Operated using any described device in claim 1-7, comprised the following steps：
A. the olefin samples bottle of more than two is respectively put into two olefin samples gas generating means 2 of more parallel, is set
The heating-up temperature and gas flow of olefin samples gas generating means 2, the olefin samples gas that two more parallels are opened respectively are filled
2 the first mass flow controller 7 is put, certain density each olefin component sample gas are respectively obtained；The alkene sample of more than two
The one kind in alkene isomer to be detected is contained with product bottle respectively, and is held respectively in the olefin samples bottle of more than two
There is alkene isomer to be detected different；
B. setting is passed through the gas flow and size of current of ozone generating-device 1, prepares ozone；
C. each olefin component sample gas for step A being obtained respectively with ozone in ozonolysis reactions device 3 hybrid reaction,
The feature spectrogram of each olefin component is obtained using reaction stream outlet detecting system 5 simultaneously；
D. the olefin samples bottle that alkene admixture of isomeric compound to be detected will be contained with is respectively put into an olefin samples gas generation
In device 2, the first mass flow controller 7 of olefin samples gas generating means 2 is opened；
E. the size of the second mass flow controller 16 is set, above-mentioned steps D part gaseous mixtures is anti-in ozone decomposed with ozone
Hybrid reaction in device 3 is answered, while obtaining the feature spectrogram of olefine mixing gas using reaction stream outlet detecting system 5；
The sample gas concentration of each olefin component for F. being obtained using weight method determination step A, and it is calculated what step D was obtained
Olefine mixing gas concentration；
G. characteristic ion species and intensity based on each olefin component, quantitative calculating is carried out to each component in mixture.
The gas conduit 9 is quartz capillary or stainless steel capillary；
The ozonolysis reactions device 3 is the pipeline of stainless steel, and non-cohesive material, it is to avoid ozone is to reaction pipeline
Corrosion.
Reaction stream outlet detecting system 5 is online gas sampling mass spectrograph, and reaction stream outlet is entered using Single-photon ionization (SPI)
Row ionization, the method can simplify the spectrogram of ozonolysis product, be easy to spectrum elucidation.
Wherein, the flow that the ozone concentration that ozone generating-device is produced can occur electric current and pure oxygen high by adjusting is adjusted.
Ozonolysis reactions device uses internal diameter about 4mm, the U-shaped stainless steel tube of length about 0.8m, olefin samples gas mixing arrangement
Using internal diameter about 2mm, the screw type stainless steel tube of 0.5m is about.In addition, reaction stream outlet detecting system uses single photon
The time of-flight mass spectrometer of ionization, the mass spectrograph is designed using orthogonal acceleration, is detected with MCP detectors, reaction stream outlet
A part is analyzed by the capillary one end being connected with the ozonolysis reactions device port of export into mass spectrograph, and remaining is used as useless
Gas is discharged.Wherein, the air pressure of ionized region can be adjusted by changing the internal diameter and length of capillary.Ionized region is total in experiment
Air pressure maintains 30Pa or so.
Embodiment 1
For the examination of the system and method performance of each component in a kind of quantitative analysis alkene admixture of isomeric compound of the present invention,
Experiment is quickly existed with 1- octenes, three kinds of isomers of cis-2- octenes and cis-3- octenes as object using the quantified system analysis
Line obtains three kinds of feature spectrograms of octene ozonolysis product, so that it is determined that its characteristic ion peak.Wherein, filled into ozone
The high-purity O for putting2Flow be 3.3L/min, generations electric current be 0.6A.The sample of 1- octenes, cis-2- octenes and cis-3- octenes
Gas generating means is respectively at 100 DEG C, 80 DEG C, 60 DEG C, by three kinds of high-purity O of octene sample gas generating means2Flow is equal
It is 700ml/min.During the gaseous mixture of online three kinds of octenes of preparation, the 700ml/min of three kinds of octene biased sample gas enters ozone
Decomposition reaction apparatus and ozone hybrid reaction, remaining is discharged as waste gas.The ionization mode of ionization source uses VUV in experiment
Single-photon ionization (VUV-SPI), ionized region air pressure maintains 30Pa or so, and the sampling time is 15s.Fig. 2 is three kinds pungent
The feature spectrogram of alkene ozonolysis product, Fig. 3 (a) is the feature spectrogram of its gaseous mixture ozonolysis product.It can be found that
The ozonolysis product spectrogram of three kinds of isomers is widely different, have uniqueness characteristic ion peak, but also have identical feature from
There is m/z=72 quasi-molecular ions at sub- peak, such as 1- octenes and cis-2- octenes, and cis-2- octenes and cis-3- octenes have m/z=57,58
Quasi-molecular ions with 59.Therefore, in order to each component accurate quantitative analysis in gaseous mixture, write a quantitative analysis procedure, utilize
Various features quasi-molecular ions is to each component accurate quantitative analysis.Fig. 4 (a) is to above-mentioned gaseous mixture using quantitative analysis procedure and weight method
Each component carries out quantitative result, compares and finds that the relative amount deviation of each alkene is 1.2%~2.5%, therefore using this quantitative point
Analysis system and method have accuracy higher.
Embodiment 2
For the examination of the system and method performance of each component in a kind of quantitative analysis alkene admixture of isomeric compound of the present invention,
Experiment is quickly existed with 1- octenes, three kinds of isomers of cis-2- octenes and cis-3- octenes as object using the quantified system analysis
Line obtains three kinds of feature spectrograms of octene ozonolysis product, so that it is determined that its characteristic ion peak.Wherein, filled into ozone
The high-purity O for putting2Flow be 3.3L/min, generations electric current be 0.6A.The sample of 1- octenes, cis-2- octenes and cis-3- octenes
Gas generating means is respectively at 120 DEG C, 80 DEG C, 60 DEG C, by three kinds of high-purity O of octene sample gas generating means2Flow is equal
It is 700ml/min.During the gaseous mixture of online three kinds of octenes of preparation, the 700ml/min of three kinds of octene biased sample gas enters ozone
Decomposition reaction apparatus and ozone hybrid reaction, remaining is discharged as waste gas.The ionization mode of ionization source uses VUV in experiment
Single-photon ionization (VUV-SPI), ionized region air pressure maintains 30Pa or so, and the sampling time is 15s.Fig. 2 is three kinds pungent
The feature spectrogram of alkene ozonolysis product, Fig. 3 (b) is the feature spectrogram of its gaseous mixture ozonolysis product.It can be found that
The ozonolysis product spectrogram of three kinds of isomers is widely different, have uniqueness characteristic ion peak, but also have identical feature from
There is m/z=72 quasi-molecular ions at sub- peak, such as 1- octenes and cis-2- octenes, and cis-2- octenes and cis-3- octenes have m/z=57,58
Quasi-molecular ions with 59.Therefore, in order to each component accurate quantitative analysis in gaseous mixture, write a quantitative analysis procedure, utilize
Various features quasi-molecular ions is to each component accurate quantitative analysis.Fig. 4 (b) is to above-mentioned gaseous mixture using quantitative analysis procedure and weight method
Each component carries out quantitative result, compares and finds that the relative amount deviation of each alkene is 0.2%~1.4%, therefore using this quantitative point
Analysis system and method have accuracy higher.
Claims (10)
1. in a kind of quantitative analysis alkene admixture of isomeric compound each component device, it is characterised in that：Exist including gaseous mixture
Line preparation system, olefinic double bonds oxidative system and reaction stream outlet detecting system (5)；
The online preparation system of gaseous mixture includes feeder (4), olefin samples gas generating means (2) and olefin samples gas
Mixing arrangement (17), olefinic double bonds oxidative system includes ozone generating-device (1) and ozonolysis reactions device (3)；
Wherein, feeder (4) includes oxygen source (6), and the gas vent of oxygen source (6) occurs with ozone respectively
The gas access of device (1) is connected with the carrier gas inlet of two olefin samples gas generation device (2) of more parallel, and in oxygen
Every between gas source of the gas (6) and ozone generating-device (1) and two olefin samples gas generation device (2) of more parallel
The first mass flow controller (7) is equipped with pipeline；
The ozone outlet of ozone generating-device (1) is connected with the gas access of ozonolysis reactions device (3), more than two
The gas vent of olefin samples gas generating means (2) in parallel be connected after through olefin samples gas mixing arrangement (17) and second
Mass flow controller (16) is connected with the gas access of ozonolysis reactions device (3), ozonolysis reactions device (3)
The gas sampling mouthful of gas vent and reaction stream outlet detecting system (5) be connected.
2. in a kind of quantitative analysis alkene admixture of isomeric compound according to claim 1 each component device, it is special
Levy and be：
The ozonolysis reactions device (3) is copper pipe or stainless steel tube, and its one end goes out with the ozone of ozone generating-device (1)
Gas port is connected with the gas vent of olefin samples gas generating means (2), the gas of the other end and reaction stream outlet detecting system (5)
Body injection port is connected；
The olefin samples gas generating means (2) at least two, is a hollow airtight cavity with heating element heater, in
What empty airtight cavity was provided with fluid sample bottle is removed and placed into mouth, and fluid sample bottle is removed and placed into mouth and can be opened by one
Closed with the lid closed, fluid sample bottle is placed in hollow airtight cavity.
3. device according to claim 2, it is characterised in that：
Ozonolysis reactions device (3) adjustable length, profile is screw type or U-shape structure, is easy to ozone with alkene long
Hydrocarbon samples gas is sufficiently mixed reaction；
Heating element heater is electrical heating wire, heat tape or electrical heating block；
Olefin samples gas generating means (2) is the stainless steel cylinder with stainless steel bottle cap, and stainless steel bottle cap and stainless steel body are logical
Screw thread fastening is crossed, and sealing is enclosed using O, inside holds fluid sample bottle.
4. device according to claim 1, it is characterised in that：
Oxygen source (6) is the dry air after steel cylinder or purification equipped with oxygen；
Ozone generating-device (1) is pure oxygen high or dry air for producing the unstripped gas of ozone gas, and the concentration of ozone is obtained
Can be adjusted by the uninterrupted of the size of current and unstripped gas that adjust corona discharge type ozone generating-device (1).
5. device according to claim 1, it is characterised in that：
The reaction stream outlet detecting system (5) is the analytical equipment of direct gas sampling, predominantly the online matter of gas sampling
Spectrometer, is connected by gas sampling pipe (9) with ozonolysis reactions device (3)；To one of ozonolysis reactions outflow gas
Divide sampling analysis, remaining is discharged as tail gas (15).
6. device according to claim 2, it is characterised in that：
The cavity size of the olefin samples gas generating means (2) can be with the size adjustment of olefin samples bottle, cavity heating-up temperature
Can be set according to the concentration of required alkene.
7. device according to claim 1, it is characterised in that：
The olefin samples gas mixing arrangement (17) is copper pipe or stainless steel tube, and adjustable length is spiral-shaped structure, is easy to same
Isomeric olefine sample gas are divided to be sufficiently mixed；
Isomerism olefin samples gas be sufficiently mixed after through the second mass flow controller (16) shunting, be partly into ozone
Decomposition reaction apparatus (3), remaining is discharged as tail gas (15).
8. a kind of any described devices of claim 1-7 each component in quantitative analysis alkene admixture of isomeric compound was analyzed
The application of journey, it is characterised in that：
Operated using any described device in claim 1-7, comprised the following steps：
A. the olefin samples bottle of more than two is respectively put into two olefin samples gas generating means (2) of more parallel,
The heating-up temperature and gas flow of setting olefin samples gas generating means (2), open two olefin samples of more parallel respectively
First mass flow controller (7) of gas generating means (2), respectively obtains certain density each olefin component sample gas；Two
It is contained with one kind in alkene isomer to be detected in olefin samples bottle more than individual respectively, and the alkene sample of more than two
It is different that alkene isomer to be detected is contained with respectively in product bottle；
B. setting is passed through the gas flow and size of current of ozone generating-device (1), prepares ozone；
C. mixing is anti-in ozonolysis reactions device (3) with ozone respectively for each olefin component sample gas for step A being obtained
Should, while obtaining the feature spectrogram of each olefin component using reaction stream outlet detecting system (5)；
D. the olefin samples bottle that alkene admixture of isomeric compound to be detected will be contained with is respectively put into an olefin samples gas generation
In device (2), first mass flow controller (7) of olefin samples gas generating means (2) is opened；
E. the size of the second mass flow controller (16) is set, by above-mentioned steps D part gaseous mixtures and ozone in ozone point
Solution reaction unit (3) interior hybrid reaction, while obtaining the characteristic spectrum of olefine mixing gas using reaction stream outlet detecting system (5)
Figure；
The sample gas concentration of each olefin component for F. being obtained using weight method determination step A, and it is calculated what step D was obtained
Olefine mixing gas concentration；
G. characteristic ion species and intensity based on each olefin component, quantitative calculating is carried out to each component in mixture.
9. application according to claim 8, it is characterised in that：
The gas conduit (9) is quartz capillary or stainless steel capillary；
The ozonolysis reactions device (3) is the pipeline of stainless steel, and non-cohesive material, it is to avoid ozone is to reaction tube
The corrosion on road.
10. application according to claim 8, it is characterised in that：
Reaction stream outlet detecting system (5) is online gas sampling mass spectrograph, and reaction is flowed out using Single-photon ionization (SPI)
Gas is ionized, and the method can simplify the spectrogram of ozonolysis product, be easy to spectrum elucidation.
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